Method for rapid maturation of distilled spirits using light and heat processes

ABSTRACT

An improved system and process for rapidly producing distilled spirits having characteristics associated with a much longer maturation process is provided. The method involves contacting wood with an unmatured distilled spirit under heated conditions and contacting the resulting heat-treated spirit with actinic light. The disclosure provides embodiments where a spirit is sequentially processed through heat and actinic light treatment. The disclosure also provides embodiments where a heat-treated spirit is mixed with a spirit that has been separately treated with light to give characteristics of a mature spirit. Air may also be percolated through a mature spirit in a container with a headspace at a gauge pressure between about −25 inHg and about −30 inHg, until the alcohol concentration of the mature spirit is reduced by between about 1% to about 2% by volume, and until the total volume of the mature spirit is reduced by about 10% or less.

CROSS-REFERENCE TO RELATED APPLICATION

This application is a divisional application of U.S. Ser. No.15/583,993, filed May 1, 2017; which is a continuation-in-part of U.S.Ser. No. 14/795,841, filed Jul. 9, 2015, now U.S. Pat. No. 9,637,713,issued May 2, 2017; which is a continuation-in-part of U.S. Ser. No.14/594,944, filed Jan. 12, 2015, now U.S. Pat. No. 9,637,712, issued May2, 2017, which is a continuation-in-part of U.S. Ser. No. 14/152,915,filed Jan. 10, 2014, now abandoned. Each disclosure of is herebyincorporated by reference in its entirety.

TECHNICAL FIELD

The technical fields are: Food Chemistry and Other Consumer Goods.

BACKGROUND ART

By some accounts, human beings have been aging distilled spirits inwooden containers for almost five hundred years. Despite billions ofperson-hours of experience, the myriad of chemical reactions responsiblefor the flavor of wood-aged spirits are not fully understood. Spiritsderive their distinct characteristics over time while stored in woodencontainers in part by the production and presence of esters. Esters arecompounds made by chemically bonding acid molecules and alcoholmolecules to form new compounds, often with pleasant aromas and tastes.This process is known as “esterification.” In addition toesterification, wood-aged spirits derive additional characteristicsthrough other processes, including extraction of flavor compounds fromthe wood container (e.g., the ubiquitous oak barrel). These processesare not necessarily separate or distinct, and can interact with andaffect each other.

Spirits also derive their distinct characteristics over time whilestored in wooden containers in part from the quicker evaporation of morevolatile organic compounds (VOCs) through the barrel walls, over theslower evaporation of other organic compounds. The aging process thuseliminates some undesired compounds, such as methanol, and concentratesand rebalances others, such as flavorful esters formed from reactionswith the wood barrel.

Attempts have been made to accelerate maturation of distilled spirits bycycling or varying pressures over relatively large ranges (e.g., between−2 and 10 ATM; see U.S. Patent Publication No. 2013/0149423). Theseprocesses generally do not yield a product close enough to that producedby traditional means. Other environmental conditions are more importantto achieve characteristics associated with a mature flavor.

Consumers of distilled spirits are often educated and discerning. Manywill refuse to consume or pay a premium for non-authentic tastingproducts. What is needed is a means by which the quality andcomplexities associated with traditionally aged spirits can be achievedin a significantly reduced timeframe, sometimes with a reduction in theevaporation of finished goods and a reduction of the build-up of ethylacetate.

SUMMARY

The following embodiments and aspects thereof are described andillustrated in conjunction with systems, tools and methods which aremeant to be exemplary and illustrative, not limiting in scope. Invarious embodiments, one or more of the above-described problems havebeen reduced or eliminated, while other embodiments are directed toother improvements.

Briefly, therefore, one aspect of the present disclosure encompasses aprocess for producing a mature spirit comprising (a) providing heat to amixture consisting essentially of an unmatured distilled spirit andwood, to maintain a temperature between about 140° F. and about 170° F.for a period of time ranging from about 24 hours to about 336 hours togive a distilled spirit mixture; then (b) contacting the distilledspirit mixture with wood and actinic light at a wavelength spectrumranging from 400 nm to 1000 nm for at least two hours to give an actiniclight-treated distilled spirit mixture; and then (c) providing heat tothe actinic light-treated distilled spirit mixture produced in step (b)to maintain a temperature between about 140° F. and about 170° F. for aperiod of time ranging from about 12 hours to about 336 hours to producethe mature spirit; and the wherein steps (a), (b), and (c) are performedsequentially.

Another aspect of the present disclosure encompasses a process forproducing a mature spirit comprising: (a) providing heat to a mixtureconsisting essentially of an unmatured distilled spirit and wood, tomaintain a temperature between about 140° F. and about 170° F. for aperiod of time ranging from about 24 hours to about 336 hours to give adistilled spirit mixture; then (b) contacting the distilled spiritmixture with wood and actinic light at a wavelength spectrum rangingfrom 400 nm to 1000 nm for at least two hours to give an actiniclight-treated distilled spirit mixture; then (c) providing heat to theactinic light-treated distilled spirit mixture produced in step (b) tomaintain a temperature between about 140° F. and about 170° F. for aperiod of time ranging from about 12 hours to about 336 hours to producethe mature spirit; and then (d) percolating air through the maturespirit of step (c) in a container with a headspace at a gauge pressurebetween about −25 inHg and about −30 inHg until alcohol concentration ofthe mature spirit is reduced by between about 1% and about 2% by volume,and until the total volume of the mature spirit is reduced by about 10%or less; wherein steps (a), (b), (c), and (d) are performedsequentially.

The unmature distilled spirit may be selected from the group consistingof sugar cane spirits, grain spirits, fruit spirits, or agave spirits.The unmature distilled spirit also be selected from the group consistingof rum, tequila, mescal, whiskey, brandy, gin, and vodka.

The concentration in the mature spirit may be decreased for one or morechemical markers selected from the group consisting of methanol, C₂-C₆fatty acids, and C₂-C₆ fatty acid esters, such as ethyl acetate. Theconcentration in the mature spirit may be increased for one or morechemical markers selected from the group consisting of vanillin,phenylated esters, C₇-C₂₄ fatty acid esters, and phenolic aldehydes. Forexample, the mature spirit may characterized by an increase inconcentration of sinapaldehyde, ethyl dodecanoate, and ethyl decanoate,such as an increase in concentration of sinapaldehyde. In particular,the mature spirit may be characterized by amounts of sinapaldehyde,ethyl dodecanoate, and ethyl decanoate that are substantially similar tothe relative proportions shown in FIG. 6, as measured by GCMS. Themature spirit may have an ethyl acetate concentration of about 59,000μg/L.

Steps (a) and (c) are maintained at a temperature between about 140° F.and about 150° F. for a period of time ranging from about 168 hours toabout 226 hours. Alternatively, steps (a) and (c) are maintained at atemperature between about 150° F. and about 160° F. for a period of timeranging from about 24 hours to about 72 hours. The process may furthercomprise (e) contacting the mature spirit of step (c) with wood andactinic light at a wavelength spectrum ranging from 400 nm to 1000 nmfor at least two hours. The process may also further comprise (f)heating with wood at a temperature between about 140° F. and about 170°F. for a period of time ranging from about 24 hours to about 336 hoursafter step (e).

The alcohol concentration of the mature spirit may be determined duringthe process using an in-line density meter connected to the container.The gauge pressure may be between about −27 inHg and about −28 inHg,such as about −27.75 inHg. The temperature of the mature spirit may beheld constant during step (d). The mature spirit in step (d) may beginwith an alcohol concentration between about 60% and about 95.5% byvolume. The process may further comprise (g) diluting the mature spiritof step (d) with water to an alcohol concentration between about 50% andabout 55% by volume, and then (h) percolating air through the dilutedmature spirit in the container with the headspace at a gauge pressurebetween about −25 inHg and about −30 inHg until the alcoholconcentration of the diluted mature spirit is reduced by an additionalamount of between about 0.3% and about 1% by volume. The temperature ofthe mature spirit may also be held constant during the step (h).

In some embodiments, the disclosure provides a process comprising: (a)contacting an unmature distilled spirit with wood and actinic light at awavelength spectrum ranging from 400 nm to 1000 nm for at least twohours to give an actinic light-treated distilled spirit mixture; then(b) providing heat to a mixture consisting essentially of the actiniclight treated spirit mixture and wood, to maintain a temperature betweenabout 140° F. and about 170° F. for a period of time ranging from about24 hours to about 336 hours; and then (c) percolating air through themature spirit of step (c) in a container with a headspace at a gaugepressure between about −25 inHg and about −30 inHg until alcoholconcentration of the mature spirit is reduced by between about 1% toabout 2% by volume, and until the total volume of the mature spirit isreduced by about 10% or less.

In other embodiments, the present disclosure provides a processcomprising: (a) contacting an unmature distilled spirit with wood andactinic light at a wavelength spectrum ranging from 400 nm to 1000 nm togive an actinic light-treated distilled spirit mixture; and then (b)contacting the actinic-light treated spirit mixture and wood at atemperature between about 140° F. and about 170° F. for a period of timeranging from about 24 hours to about 336 hours; and then (c) percolatingair through the mature spirit of step (b) in a container with aheadspace at a gauge pressure between about −25 inHg and about −30 inHguntil alcohol concentration of the mature spirit is reduced by betweenabout 1% to about 2% by volume, and until the total volume of the maturespirit is reduced by about 10% or less.

The present disclosure also provides a process for producing a maturespirit comprising: (a) providing heat to a mixture consistingessentially of an unmatured distilled spirit and wood, to maintain atemperature between about 140° F. and about 170° F. for a period of timeranging from about 24 hours to about 336 hours to give a distilledspirit mixture; (b) contacting the distilled spirit mixture with woodand actinic light at a wavelength spectrum ranging from 400 nm to 1000nm for at least two hours to give an actinic light-treated distilledspirit mixture; (c) providing heat to the actinic light-treateddistilled spirit mixture produced in step (b) to maintain a temperaturebetween about 140° F. and about 170° F. for a period of time rangingfrom about 12 hours to about 336 hours to produce the mature spirit; and(d) percolating air through the mature spirit of step (c) in a containerwith a headspace at a gauge pressure between about −25 inHg and about−30 inHg until alcohol concentration of the mature spirit is reduced bybetween about 1% to about 2% by volume, and until the total volume ofthe mature spirit is reduced by about 10% or less; wherein the wood hasbeen washed with a solution of carboxylic acid in water prior to step(a), and wherein steps (a), (b), (c), and (d) are separate andsequential.

The present disclosure also provides a process comprising: (a)contacting an unmature distilled spirit with wood and actinic light at awavelength spectrum ranging from 400 nm to 1000 nm for at least twohours to give an actinic light-treated distilled spirit mixture; then(b) providing heat to a mixture consisting essentially of the actiniclight treated spirit mixture and wood to maintain a temperature betweenabout 140° F. and about 170° F. for a period of time ranging from about24 hours to about 336 hours, and then (c) percolating air through themature spirit of step (b) in a container with a headspace at a gaugepressure between about −25 inHg and about −30 inHg until alcoholconcentration of the mature spirit is reduced by between about 1% toabout 2% by volume, and until the total volume of the mature spirit isreduced by about 10% or less; wherein the wood has been washed with asolution of carboxylic acid in water prior to step (a), and whereinsteps (a), (b), and (c) are separate and sequential.

Moreover, the present disclosure provides a process comprising: (a)contacting an unmature distilled spirit with wood at a temperaturebetween about 140° F. and about 170° F. for a period of time rangingfrom about 24 hours to about 336 hours to give a distilled spiritmixture; (b) contacting the distilled spirit mixture with wood andactinic light at a wavelength spectrum ranging from 400 nm to 1000 nm;and (c) percolating air through the mature spirit of step (b) in acontainer with a headspace at a gauge pressure between about −25 inHgand about −30 inHg until alcohol concentration of the mature spirit isreduced by between about 1% to about 2% by volume, and until the totalvolume of the mature spirit is reduced by about 10% or less; wherein thewood has been washed with a solution of carboxylic acid in water priorto step (a), and wherein steps (a), (b), and (c) are separate andsequential.

Additional embodiments and features are set forth in part in thedescription that follows, and in part will become apparent to thoseskilled in the art upon examination of the specification, or may belearned by the practice of the embodiments discussed herein. A furtherunderstanding of the nature and advantages of certain embodiments may berealized by reference to the remaining portions of the specification andthe drawings, which forms a part of this disclosure.

BRIEF DESCRIPTION OF THE DRAWINGS

The disclosure will be readily understood by the following detaileddescription in conjunction with the accompanying drawings, wherein likereference numerals designate like structural elements. The drawingsprovide exemplary embodiments or aspects of the disclosure and do notlimit the scope of the disclosure.

FIG. 1 shows the gas chromatograph mass spectrometry (GCMS) chromatogramfrom an unprocessed rum sample.

FIG. 2 shows the GCMS chromatogram from a sample of a commerciallyavailable rum which has been aged for 33 years by conventional agingtechniques.

FIG. 3 shows the GCMS chromatogram from a rum sample that was subjectedto heating in accordance with Example 3 but was not subjected to actiniclight.

FIG. 4 shows the GCMS chromatogram from a rum sample subjected toactinic light but not to heat in accordance with Example 4.

FIG. 5 shows the GCMS chromatogram from a rum sample that is a mixtureof rum subjected to heat and rum subjected to actinic light inaccordance with Example 5.

FIG. 6 shows the GCMS chromatogram from a rum sample that has beenprocessed with both heat and light in accordance with Example 6.

FIG. 7 depicts a wooden barrel for the heat process with a cutaway toshow the barrel's internals.

FIG. 8 depicts a sealed vessel for the heat process with a cutaway toshow the vessels internals.

DETAILED DESCRIPTION

The disclosure pertains to processes for producing a distilled spirithaving characteristics associated with a mature distilled spirit. Thedistilled spirit produced in accordance with the process has many of thecharacteristics associated with a matured distilled spirit produced inaccordance with industry standards, but is advantageously produced in ashortened timeframe while eliminating the evaporation problem andgreatly reducing the “off flavors” associated with excess ethyl acetate.By contacting an unmatured distilled spirit with wood at increasedtemperatures and contacting the spirit with actinic light, thematuration process can be shortened without reducing the quality of thespirit. In particular, it has surprisingly been found that the processesdescribed herein produce a spirit having similar chemical markers as a33-year-old spirit in a significantly reduced period of time.

This disclosure pertains also to processes for producing a distilledspirit having characteristics associated with a mature distilled spirit.The distilled spirit produced in accordance with the process has many ofthe characteristics associated with a matured distilled spirit producedin accordance with industry standards, but is advantageously produced ina shortened timeframe while reducing the evaporation problem and greatlyreducing the “off flavors” associated with excess volatile organiccompounds (VOCs), such as methanol and ethyl acetate. By percolating airthrough a distilled spirit in a container with a headspace at a gaugepressure between about −25 inHg and about −30 inHg until the alcoholconcentration of the distilled spirit is reduced by between about 1% andabout 2% by volume, and until the total volume of the distilled spiritis reduced by about 10% or less, the concentration of unwanted chemicalmarkers is decreased and the concentration of desired chemical markersis increased, without the drastic volume losses associated withtraditional aging.

The distilled spirit in step (a) may begin with an alcohol concentrationgreater than 60% by volume, and the process may then further comprise(b) diluting the distilled spirit of step (a) with water to an alcoholconcentration between about 50% and about 55% by volume, and then (c)percolating air through the diluted distilled spirit in the containerwith the headspace at a gauge pressure between about −25 inHg and about−30 inHg until the alcohol concentration of the diluted distilled spiritis reduced by an additional amount of between about 0.3% and about 1% byvolume.

Additional embodiments and features are set forth in part in thedescription that follows, and in part will become apparent to thoseskilled in the art upon examination of the specification, or may belearned by the practice of the embodiments discussed herein. A furtherunderstanding of the nature and advantages of certain embodiments may berealized by reference to the remaining portions of the specification,the drawings, the chemical structures, and descriptions, which forms apart of this disclosure. Any description of any R-group or chemicalsubstituent, alone or in any combination, may be used in any chemicalformula described herein, and formulae include all conformational andstereoisomers, including diastereomers, epimers, and enantiomers.Moreover, any feature of a composition disclosed herein may be used incombination with any other feature of a composition disclosed herein.

As used herein, a spirit refers to any distilled spirit. In particularembodiments, the spirit is a sugar cane-based, grain-based, fruit-based,or agave-based spirit, such as rum, tequila, mescal, whiskey, brandy,gin, vodka, or combinations thereof. The distilled spirit may be a sugarcane-based spirit, such as rum. The distilled spirit may be agrain-based spirit, such as whiskey, bourbon, or scotch. The distilledspirit may be a fruit-based, such as brandy. The distilled spirit may bean agave-based spirit, such as tequila or mescal. The distilled spiritmay be rum. The distilled spirit may be tequila. The distilled spiritmay be mescal. The distilled spirit may be whiskey. The distilled spiritmay be brandy. The distilled spirit may be gin. The distilled spirit maybe vodka.

The spirit may be newly distilled or it may have already undergone astandard or accelerated aging process. For example, a 15-year whiskeymay be treated as disclosed herein to produce a whiskey having a 20-yearor 30-year chemical profile. In other words, when a process disclosedherein is applied to aged spirits, the ratios of chemical markers arealtered and make the distilled spirit appear much older than it is. Theprocess works on any spirit, including un-aged spirits such as vodka,gin, un-aged rum, un-aged tequila, un-aged brandy (eau de vie), and thelike. Here, the process removes the sensation alcohol burn and tracemethanol.

A distilled spirit having the characteristics associated with a matureddistilled spirit, as used herein, describes a spirit, which, by one ormore chemical markers, has attained characteristics associated withspirits aged in accordance with industry standards. Such standards, forexample, include aging a spirit in wood over a period of time greaterthan 1, 5, 10, 15, 20, 25 or 30 years. The characteristics associatedwith a matured distilled spirit may include taste, aroma, and bodyprofiles, such as smoothness.

As used herein, lux hours refers to the amount of light exposure in agiven hour. Specifically, cumulative lux hours can be defined as howmuch energy from light should be provided over a specified period oftime.

The disclosed process rapidly removes undesired chemical markers andconcentrates desired chemical markers. A mature distilled spirit havingthe characteristics associated with a matured distilled spirit, as usedherein, describes a spirit, which has attained a flavor and aromaprofile organoleptically similar to spirits aged with wood for manyyears, and typically showing a chemical profile containing key chemicalmarkers in particular proportions.

Traditionally, producing wood-aged distilled spirits has includedcarboxylic acid esterification, phenolic acid esterification, and theformation of complex esters, including both phenolic and carboxylicacids. Carboxylic acid esters are responsible for the fruity aromas andtastes in distilled spirits. Carboxylic precursor acids are derived fromthe yeast and bacteria during fermentation. If organic materials areused for the container in which these reactions occur, those materialsalso influence the process. For example, where a charred or toasted oakbarrel is used, carboxylic precursor acids are also derived from thermaldecomposition of the oak polymer, hemi-cellulose, found in the innerlining of the barrel.

Off-flavors are various flavorful or aromatic compounds present inspirits that are often described by connoisseurs using colorful terms(e.g., “sulfury”, “solventy”, “meaty”, “acidic”, “metallic”, “vegetal”,etc.). Carboxylic precursor acids are largely responsible for“off-flavors” in distilled spirits. Another common flaw with asolvent-like “off flavor” is produced by build-up of ethyl acetate inthe maturing spirit. Other compounds, such as methanol, may not impactflavor but do diminish the consumers' enjoyment of the distilled spirit.

The disclosed process favors the removal of methanol above othercompounds present in distilled spirits. Previously known methods werevery costly to remove methanol from distilled spirits. Methanol ispartly responsible for hangovers and its removal is critical forconsumer quality perceptions. Without wishing to be bound by theory,methanol is removed from the distilled spirit as its azeotrope oreutectic. When a second sequential negative pressure treatment is used,the distilled spirits are diluted with water to bottling strength,thereby changing the azeotropic distribution within the spirits. Themethod may also remove the perception of heat in all types of spirits.This is something consumers use to perceive quality in distilledspirits.

Historically, ethyl acetate concentration was used as a marker for theprogress of aging where higher amounts indicate greater maturation time.But, ethyl acetate is not itself desirable and adds a flavor and aromacomparable to paint thinners. Moreover, samples of distilled spiritsreceiving high reviews, comparable or in some cases better than an agedspirit, do not always have a high ethyl acetate concentration. Usingmodern techniques, highly prized spirits can be analyzed for theirchemical make-up. Using these data, chemical markers can be selected asa model for a mature spirit. Surprisingly, these chemical markersprovide advantages over the traditional measurement of ethyl acetateconcentration to determine age. In particular, the chemical markers setforth herein are desirable for modeling purposes because, unlike ethylacetate, the chemical markers contribute to the desired flavor profile.In one embodiment, ethyl acetate concentrations are reduced to aconcentration less than about 200,000 μg/L. In another embodiment, theethyl acetate concentrations range between about 50,000 μg/L and about170,000 μg/L.

Fatty acids are structurally simple and even with their derivatives canbe subdivided into well-defined families. Among straight-chain fattyacids, the simplest are referred to as saturated fatty acids. They haveno unsaturated linkages in the carbon backbone and cannot be alteredduring hydrogenation or halogenation process. Saturated fatty acids tendto be solid at room temperature and their melting points increase withincreasing chain length.

The fatty acid chain lengths may range between 2 and 80 carbon atoms,and commonly between 12 and 24 carbons. With a chain length between 2and 6 carbon atoms, the fatty acids are called short-chained fattyacids, or C₂-C₆ acids. Examples of suitable short-chain fatty acidsinclude, but not limited to, formic acid, acetic acid, proprionic acid,butyric acid, isobutyric acid, valeric acid, and isovaleric acid. C₂-C₆fatty acid esters include the C₂ fatty acid ester ethyl acetate.

With a chain length from 6 to 12 carbon atoms, the fatty acids arecalled medium-chained fatty acids, or C₆-C₁₂ fatty acids. A commonsubgroup of medium-chained fatty acids is C₈-C₁₀ fatty acids, having 8to 10 carbon atoms in the chain. Examples of suitable medium-chain fattyacids include, but are not limited to, caproic acid (C₆), enanthic acid(C₇), caprylic acid (C₈), pelargonic acid (C₉), capric acid (C₁₀),undecylic acid (C₁₁), and lauric acid (Cu).

With a chain length between 12 and 24, the fatty acids are called along-chained fatty acids, or C₁₂-C₂₄ fatty acids. The same chain lengthranges apply to fatty acid derivatives, such as fatty acid esters.Examples of suitable long-chain fatty acids include, but are not limitedto, tridecylic acid (C₁₃), myristic acid (C₁₄), pentadecanoic acid(C₁₅), palmitic acid (C₁₆), margaric acid (C₁₇), stearic acid (C₁₈),nonadecylic acid (C₁₉), arachidic acid (C₂₀), and heneicosylic acid(C₂₁).

The fatty acids may be unsaturated, such as an ω-3 unsaturated fattyacid, for example, α-linolenic acid (18:3), stearidonic acid (18:4),eicosapentaenoic acid (20:5), and docosahexaenoic acid (22:6); an ω-6unsaturated fatty acid, for example, linoleic acid (18:2), γ-linolenicacid (18:3), dihomo-γ-linolenic acid (20:3), arachidonic acid (20:4),and adrenic acid (22:4); an ω-7 unsaturated fatty acid, for example,palmitoleic acid (16:1), vaccenic acid (18:1), and paullinic acid(20:1); or an ω-9 unsaturated fatty acid, for example, oleic acid(18:1), elaidic acid (trans-18:1), gondoic acid (20:1), erucic acid(22:1), nervonic acid (24:1), and mead acid (20:3).

Fischer esterification of fatty acids and alcohol is a well-understoodand commonly practiced chemical reaction. A typical laboratory processinvolves heating a solution of fatty acids and alcohols under reflux inthe presence of an acid catalyst. In laboratory settings, strong acids(e.g., sulfuric acid) are typically employed as the catalyst, but thiscan be incompatible with spirit making where other functional groups aresensitive to stronger acids and where chemical additives are typicallyprohibited. It has long been known that Fischer esterification can alsobe completed using weak acid catalysts, but at the expense of relativelyslow reaction rates. Where charred or toasted oak barrels are usedduring the maturation of distilled spirits, weak acids may be graduallyextracted from organic material in the walls of the barrel. It typicallytakes years for esters to accumulate using weak acid catalysts derivedfrom the barrel, although it has been observed that in warmerenvironments (i.e., modestly heated within the range of normalatmospheric conditions less than 120° F.) the process can be acceleratedsignificantly (from decades to years). This early form of acceleratedaging comes at the cost of increased evaporation from the barrel. Oftenas much as 50% of the product can be lost to evaporation.

When the alcohol component is glycerol, the fatty acid esters producedcan be monoglycerides, diglycerides, or triglycerides. Dietary fats arechemically triglycerides. Suitable examples of fatty acid estersinclude, but are not limited to, 2-arachidonoylglycerol, ascorbylpalmitate, ascorbyl stearate, cetyl myristoleate, cetyl palmitate, ethyldecadienoate, ethyl decanoate, ethyl eicosapentaenoic acid, ethylmacadamiate, ethyl octanoate, ethyl palmitate, ethylhexyl palmitate,glycerol monostearate, glyceryl hydroxystearate, glycol distearate,glycol stearate, isopropyl palmitate, monoctanoin, monolaurin,2-oleoylglycerol, polyglycerol polyricinoleate, and virodhamine.

Phenolic aldehydes also play a major role producing aromas similar tovanilla, pipe tobacco, and smoke. Phenolic aldehydes are largely derivedfrom thermally broken down oak polymers found within the inner lining ofthe barrel. Complex esters are responsible for complex honeyed aromas indistilled spirits. The complex esters are generally produced from thechemical reactions of both carboxylic and phenolic acids/aldehydes withalcohols during the time in the barrel or other container. Phenolicaldehydes are derivatives of phenol. Suitable examples of phenolicaldehydes include, but are not limited to, hydroxybenzaldehydes,protocatechuic aldehyde, vanillin, isovanillin, 2,3,4-trihydroxybenzaldehyde, sinapaldehyde(3-(4-hydroxy-3,5-dimethoxyphenyl)prop-2-enal), and syringaldehyde(4-hydroxy-3,5-dimethoxybenzaldehyde).

Wood extraction is the process that gives distilled spirits their colorand astringent “oaky” and “smoky” taste. Traditionally, this isattributed to tannins (polyphenols). Interestingly, our analysis ofmature spirits did not find significant evidence of tannins. But insteadfound myriad less complex wood derived phenols such as sinapaldehyde andsyringaldehyde. These oak-extracted compounds proved unexpectedly usefulas markers for monitoring the aging process described below.

Esterification and the extraction of wood compounds from the woodcontainer are some of the primary reactions taking place in thematuration process of distilled spirits. Because these processes runconcurrently, and often interact with or depend on each other as well asthe material and other conditions of their environment over time, it isvery difficult to deviate very far from traditional methods while stillachieving similar results. For example, rapid oak extraction may notprovide enough time for interaction with a wood container to pick upsome of the more subtle and complex flavors present in traditionallyaged spirits. Much of the expense in spirit making stems from the longlatency in creating the end product as well as the product evaporationfrom the barrel. Stock must be stored, often in climate-controlledenvironments, and tested repeatedly during maturation. But, it isdifficult to predict markets many years out. Makers that produce toomuch product fail to maximize their investment, whereas those thatproduce too little fail to capture potentially significant portions ofthe upside.

In one embodiment, a mature spirit can be characterized by thedecreasing concentrations of one or more chemical markers. Throughoperation of a process disclosed herein, the concentration in thedistilled spirit may decrease for one or more chemical markers selectedfrom the group consisting of methanol, C₂-C₆ fatty acids, and C₂-C₆fatty acid esters.

The concentration in the distilled spirit may increase for one or morechemical markers selected from the group consisting of vanillin,phenylated esters, C₇-C₂₄ fatty acid esters, and phenolic aldehydes.These things are responsible for the flavor described as the “finish” indistilled spirits. Three markers in particular, are thought to beparticularly useful for defining a mature spirit: sinapaldehyde, ethyldecanoate, and ethyl dodecanoate. Ethyl decanoate and ethyl dodecanoateare often found in unmature spirits at low concentrations. Sinapaldehydeis typically not found in an unmature spirit.

The distilled spirit may be characterized by an increase inconcentration of sinapaldehyde, ethyl dodecanoate, and ethyl decanoate.The distilled spirit may be characterized by an increase inconcentration of sinapaldehyde. In one embodiment, a mature spirit maybe characterized by an increase of at least about threefold for ethyldodecanoate over an unmature spirit. In another embodiment, a maturespirit is characterized by an increase of at least about threefold forethyl decanoate over an unmature spirit. Increased concentrations may beassessed by any method known in the art.

A spirit that presents these three compounds in relative proportion (asassessed by peak height measured by gas chromatography mass spectrometry(GCMS)) typically has desirable flavor characteristics. In this regard,a mature spirit may also be characterized by a sinapaldehyde peakgreater than 80% and less than 200% of the peak height of ethyldecanoate and ethyl dodecanoate as measured by GCMS. Without being boundto any theory, it is believed that sinapaldehyde concentration isdisproportionately important in creating a spirit that meets theorganoleptic properties of a mature spirit.

In another embodiment, a mature spirit is one that produces relativepeak heights that are substantially similar to the peak heights shown inFIG. 5 for sinapaldehyde, ethyl decanoate, and ethyl dodecanoate.“Substantially similar,” as used herein, refers to a relative peakheight differing by no more than 30%, no more than 25%, no more than20%, no more than 15%, no more than 10%, no more than 5%, or no morethan 2%. In still another embodiment, a mature spirit is one thatproduces relative peak heights that are substantially similar to therelative peak heights shown in FIG. 5 for sinapaldehyde, ethyldecanoate, ethyl dodecanoate, and acetyl. In still a further embodiment,a mature spirit is one that produces relative peak heights that aresubstantially similar to the relative peak heights shown in FIG. 5 forsinapaldehyde, ethyl decanoate, ethyl dodecanoate, acetyl, andsyringaldehyde.

In yet another embodiment, a mature spirit is one that produces relativepeak heights that are substantially similar to the relative peak heightsshown in FIG. 6 for sinapaldehyde, ethyl decanoate, and ethyldodecanoate. In still another embodiment, a mature spirit is one thatproduces relative peak heights that are substantially similar to therelative peak heights shown in FIG. 6 for sinapaldehyde, ethyldecanoate, ethyl dodecanoate, and acetyl. In yet another embodiment, amature spirit is one that produces relative peak heights that aresubstantially similar to the relative peak heights shown in FIG. 6 forsinapaldehyde, ethyl decanoate, ethyl dodecanoate, acetyl, andsyringaldehyde.

The unmatured distilled spirit is a spirit that has not attained themarkers or characteristics associated with a matured distilled spirit.The “unmatured distilled spirit,” as described herein, refers to whiteor raw spirits, as well as partially matured spirits, provided that theunmatured distilled spirit is lacking in certain characteristics of amatured spirit. The unmatured distilled spirit, as described herein, hasan alcohol content of at least 50% by volume. In some embodiments, thealcohol content of the unmature distilled spirit is between 50% and 80%by volume.

The term “distilled spirit mixture,” as used herein, refers to anydistillate on the spectrum from matured to unmatured. The term“distillate” as used herein refers to the liquid composition in thevessel and may include an unmatured distilled spirit, a matureddistilled spirit, or a distilled spirit mixture.

The unmatured distilled spirit is contacted with wood in a vessel. Inone embodiment, the wood is provided as the vessel for holding thedistillate. In such embodiments, the vessel is, for example, an oakbarrel. In other embodiments, wood may be provided to the inside of thereaction vessel, which is optionally made of wood. For example, woodchips may be added such that they are submerged or floating on top ofthe distillate. Wood may also be provided as various structuralconfigurations within the vessel including as baffles or packing. Instill other embodiments, wood may include wood extracts and raw acidsdesigned to mimic the characteristics of wood. In one embodiment, thewood is oak.

Of the various advantages of the present disclosure, one is that noadditional ingredients or acids are provided to facilitate the process.In this regard, the process is free of additives. Without being bound toany particular theory, it is thought that the inventive process rapidlyextracts acids from the wood. These acids facilitate the esterificationprocess without the need for additives beyond the wood and the unmatureddistilled spirit.

A. Sequential Temperature and Light Processing

One aspect of the present disclosure provides a process for producing amature spirit using sequential temperature and light processing. In thisregard, the process comprises the steps of (a) contacting an unmatureddistilled spirit with wood at a temperature between about 140° F. andabout 170° F. for a period of time ranging from about 24 hours to about336 hours to give a distilled spirit mixture; (b) contacting thedistilled spirit mixture with wood and actinic light having a wavelengthspectrum ranging from 400 nm to 1000 nm for at least 2 hours to give anactinic light-treated distilled spirit mixture; and (c) providing heatto the actinic light-treated distilled spirit mixture produced in step(b) to maintain a temperature between about 140° F. and about 170° F.for a period of time ranging from about 12 hours to about 336 hours toproduce the mature spirit.

(i) First Thermal Process

In the sequential process described herein, the unmatured spirit is besubjected to thermal processing. In this regard, the unmatured distilledspirit is contacted with the wood at a temperature ranging from about140° F. to about 170° F. In alternate embodiments, the temperatureranges from about 140° F. to about 150° F., from about 145° F. to about150° F., from about from about 150° F. to about 160° F., or from about160° F. to about 170° F.

The time period needed to convert the unmatured distilled spirit to adistilled spirit mixture having partial characteristics associated witha matured spirit, for example, as shown in FIG. 3, depends on factorssuch as the starting composition of the unmatured distilled spirit andthe temperature at which the process is conducted. In some embodiments,a temperature between about 140° F. and about 170° F. is provided for aperiod of time ranging from about 12 hours to about 336 hours. Inalternate embodiments, a temperature between about 140° F. and about170° F. is provided for a period of time ranging from about 12 hours toabout 24 hours, from about 24 hours to about 48 hours, from about 48hours to about 96 hours, from about 96 hours to about 168 hours, fromabout 168 hours to about 226 hours, or from about 226 hours to about 336hours.

The heating is conducted in a sealed vessel or under reflux such thatevaporation of volatile compounds is prevented. The pressure inside thevessel can and will vary in different embodiments of the disclosure. Ingeneral, the internal pressure of the vessel housing the reactioncomponents climbs to a maximum of about 6 pounds per square inch (psi).The typical range of pressures in the vessel is between 2 psi and 6 psi,but can be altered to relieve pressure and maintain an operatingpressure of less than 1 psi while still achieving the desired chemicalreactions.

In one embodiment, the temperature is maintained between about 140° F.and about 150° F. for a period of time ranging from about 168 hours toabout 226 hours.

In another embodiment, the temperature is maintained between about 150°F. and about 160° F. for a period of time ranging from about 24 hours toabout 72 hours.

Generally, heat is applied continuously through the given time period.But, heat may also be provided for the given time period in a mannerthat is not continuous, for example, at intervals so long as heat isprovided totaling the stated time period. At the end of this timeperiod, a first distilled spirit mixture is provided. In this embodimentof the disclosure, the first distilled spirit mixture produced by theheat process is further reacted as described below.

The heat process may be conducted in an apparatus as shown in FIG. 7,which shows a cutaway view of one possible internal configuration. Thevessel 1 may be a wooden barrel.

In the embodiment depicted in FIG. 8, a cutaway is shown using dashedlines to reveal another possible internal confirmation of the vessel 1,where vessel 1 may be a stainless steel container. In this embodiment,the wood 12 is provided as chips or planks submerged in or floating ontop of the distillate 2.

For both FIG. 7 and FIG. 8, heat may be applied to the distillate 2inside the vessel 1 via a heat source 4. In one embodiment, the vesselis sealed under pressure. In another embodiment, the vessel is heatedunder reflux to prevent evaporation of volatile compounds. Any methodfor introducing sufficient heat to the distillate including an internalelectrical heating element 9 may be used. In such an embodiment,temperature may be controlled by manipulating electrical current in theinternal electrical heating element 9 circuit. In alternate embodimentsthe heat source 4 is external and may be used with a conduit 16,conductor, or the like. In one non-limiting example, steam 18 may becreated using an external boiler as the heat source 4 in one embodiment,then passed through a conduit 16 running through the vessel 1, wherein aconductive portion 16 of the conduit is submerged in the distillate 2.In such an embodiment, the temperature of the distillate 2 may becontrolled by varying the amount of steam 18 produced by the boiler.Such control may be provided by valves or similar means that are notpictured.

In one embodiment, the temperature of the distillate 2 in the vessel 1is brought up to a temperature of about 160° F. for a period of up to 48hours. This process simultaneously extracts wood derived compounds andacids, some of which are thought to be esterification catalysts. In oneembodiment, the temperature of the distillate is measured via atemperature sensor 5. Any known temperature sensor may be used. Thetemperature of the distillate 2 may be controlled by manuallymanipulating the heat source 4. In an alternate embodiment, anelectronic temperature sensor is coupled 10 to a controller 7. Thecontroller 7 may be configured to present an alert (e.g., flash a light,produce a sound, produce an electrical signal, transmit a text message,e-mail or other electronic communication, etc.) when the temperature ofthe distillate 2 is outside of a provided range. Optionally, thecontroller 7 may be coupled to the heat source 4, in which case, thecontroller is configured to manipulate the heat source to keep thetemperature of the distillate 2 within the provided range.

Heating in accordance with the disclosure triggers the esterification offree volatile acids and alcohols in the distillate 2, while theheadspace 3 provides for reflux within the vessel 1 allowing any weakacids to be rapidly extracted from the wood. These weak acids, incombination with elevated temperatures, appear to help catalyze theesterification of free acids in the distillate per the Fischer process,which would otherwise take many years in traditional containers.

The pressure inside the container may be measured by a pressure sensor6. The pressure sensor 6 may be coupled to the controller 7. Thepressure sensor may be configured to provide alerts if the pressurebecomes too high. The pressure sensor may optionally be configured tocommunicate to open a release valve if the pressure is too high.

(ii) Actinic Light Process

The first distilled spirit mixture provided in step (i) is generallyallowed to cool and transferred for processing with actinic light. Inaccordance with one embodiment of the disclosure, the first distilledspirit mixture is contacted with actinic light having a wavelengthspectrum in the range of 400 nm to 1000 nm for at least 2 hours to givean actinic light-treated distilled spirit.

The actinic light process takes place in a container that allows smallamounts of light in the UV-Visible spectrum to pass through. Thequantity of UV light contacting the spirits is comparable to levelsfound in daylight, and is not thought to be contributing significantlyto the spirits maturation process but is instead incidental to theprocess. In a brief experiment, the inventor compared the UVC and UVA/Blevels found in the actinic light stream used to mature the spirits toUVC and UV A/B levels in sunlight at noon in Morgan Hill, Calif. Thelevels were evaluated using a General Instruments UV512C UVC meter and aGeneral Instruments UV513AB. The UVC levels reaching the spirits werefound to be between 10-20 μW/cm² as compared with 15 μW/cm² found in thesunlight. The combined UVA and UVB levels reaching the maturing spiritwere found to be 3500 μW/cm²+/−1000 μW/cm² as compared with 5000 μW/cm²in the measured sunlight. This experiment shows that the UV light levelsin the stream of actinic light responsible for playing a role inmaturing the spirit are no greater than sunlight, whereas the otherwavelengths are significantly higher in proportion to sunlight. Thecontainer is filled with the spirit to be processed and is alsogenerally filled with wood as described in the previous step. In oneembodiment, glass carboys are used. The actinic light may come from avariety of sources including natural, synthetic, or a combinationthereof. Generally, the exposure in this step can be at least two hours.In some embodiments, the exposure can be up to 336 hours.

In an alternative embodiment, the exposure in this step can be at least2,280,000 lux hours, but sometimes as high as 20,000,000 lux hours. Inother embodiments, the total exposure is at least 1,000,000 lux hours,at least 1,500,000 lux hours, at least 2,000,000 lux hours, at least2,500,000 lux hours, or at least 3,000,000 lux hours. Where very highconcentrations of the chemical markers described herein are sought evengreater exposures might be appropriate.

In one embodiment, the first distilled spirit mixture is exposed to theentire broad spectrum of wavelengths from 400 nm to 1000 nm. In analternative embodiment, specific wavelengths of the light found in the400 nm to 1000 nm range may be concentrated in relation to others toproduce varying effects in the maturing spirits. For example,wavelengths used may be selected from, but are not limited to, about 400nm to about 600 nm, from about 550 nm to about 650 nm, from about 600 nmto about 700 nm, from about 650 nm to about 750 nm, from about 700 nm toabout 800 nm, from about 750 nm to about 850 nm, from about 800 nm toabout 900 nm, from about 850 nm to about 950 nm, or from about 900 nm toabout 1000 nm. In particular, the wavelength may range between about 600nm and about 1000 nm. This process may also be used to isolate thewavelengths most responsible for the effects observed in the spiritmaturation process. Where specific temperatures are needed to triggerthe reactions with the actinic light, heaters may be used in conjunctionwith special lamps which produce specific wavelengths of light at aspecific temperature. Using specific wavelengths alone, or with heaters,to mature the spirit, would allow for lower energy consumption and lowertotal LUX value to accomplish the same tasks.

The time period over which the actinic light process is conducted canand will vary over different embodiments. Where natural light is used,the total exposure to actinic light may range from about 100 hours toabout 500 hours, from about 250 hours to about 750 hours, from about 500hours to about 1000 hours, from about 750 hours to about 1250 hours, orfrom about 1000 hours to about 1500 hours. Where synthetic lights areused, the total exposure to actinic light may range from about 2 hoursto about 12 hours, from about 12 hours to about 24 hours, from about 24hours to about 48 hours, from about 48 hours to about 96 hours. Ifartificial lights are used that provide a very low lux value, time isincreased proportionally to achieve the lux hour value.

The actinic light process may be conducted below the boiling point ofthe spirit. In some embodiments, the amount or duration of actinic lightis controlled, for example, by exposing the spirit to light in adiscontinuous manner, by cooling the spirits, by temporarily shieldingthe spirit from the actinic light, or by other methods for controllingtemperature that are known in the art. This process may also be carriedout under reflux to prevent the evaporation of volatile compounds.

Although pressure is not thought to be critical to the actinic lightprocessing, the actinic light processing is generally conducted atatmospheric pressures. The light processing step may accommodate higheror lower pressures.

In one embodiment, a tungsten halogen bulb is used to provide theactinic light. The bulb has an average light temperature of 2900°, andcan produce light in a broad spectrum of wavelengths, includingwavelengths from 400 nm to 1000 nm. The spirits can be exposed to thelight in a period of at least 2 hours. In at least one embodiment, thesprits are placed in clear containers where about 100 liters of spiritcover a square meter. The area is illuminated to about 190,000 lux withthe light being toggled off and on in periods of 2-4 hours to reach atotal exposure of 4,500,000 lux hours. Lux hours, as used herein,describes the light exposure in a given hour because it describes thetotal luminescence in a given time. Radiant flux measurements wereunavailable because the data was not available.

In another embodiment, a distilled spirit is placed in a translucent jarthat was kept in a greenhouse for 168 hours to achieve a total ofapproximately 4,200,000 lux hours.

In another embodiment, twenty 500-W halogen bulbs are used to providelight to seventy jars. The lights are toggled on and off for three daysto provide the total lux hours needed for the reaction.

In still another embodiment, 500-W halogen bulbs are shined on bothsides of a glass jar. The lights are toggled on and off for 14 hours toprovide the total lux hours needed for the reaction.

When the actinic light processing is complete, the resulting actiniclight-treated spirit mixture is removed from the light source.

(iii) Second Thermal Process

The sequential process further involves a temperature process conductedwith the resulting mixture from Section A(ii). In this regard, theactinic light-treated distilled spirit mixture is heated to maintain thetemperature of the actinic light-treated distilled spirit mixturebetween about 140° F. and about 170° F. for a period of time rangingfrom about 12 hours to about 336 hours in a sealed vessel or underreflux such that evaporation of volatile compounds is prevented toproduce a mature spirit.

The process of heat treating the actinic light-treated spirit isconducted in the manner described in Section A(i) except that theprocess is performed on the actinic light-treated distilled spiritmixture produced in accordance with Section A(ii). Beneficially, thisstep triggers a marked reduction in ethyl acetate concentrationsgenerated during the actinic light treatment, shown experimentally to begreater than 60%.

(iv) Optional Further Processing

Optionally, the spirit produced by the process described in SectionsA(i) through A(iii) may be followed by one or more additional actiniclight or thermal processing steps. For example, a second actinic lightprocessing step may be conducted on the product obtained by the secondthermal processing step. A third thermal processing step may also beutilized after a second actinic light processing step. In oneembodiment, the processes includes a further step of (d) of contactingthe product of step (c) with wood and actinic light at a wavelengthspectrum ranging from 400 nm to 1000 nm for at least 2 hours. In stillanother embodiment, the process further comprises the step (e) ofcontacting the product of step (d) with wood at a temperature betweenabout 140° F. and about 170° F. for a period of time ranging from about24 hours to about 336 to give a first distilled spirit mixture

In one embodiment, the sequential process may be repeated until adesired chemical marker profile is obtained.

(v) Inverted Sequential Embodiment

In still another embodiment of the present disclosure, the sequentialprocess begins with an unmature distilled spirit contacted with actiniclight as described in Section (A)(ii) to form an actinic light-treateddistilled spirit mixture. Following this treatment, the actiniclight-treated distilled spirit mixture is treated thermally as describedin Section (A)(i). These steps may be repeated until a desired flavorprofile is obtained as determined by the chemical markers describedherein.

B. Mixed Batch Process

In another embodiment, the present disclosure provides a mixed batchprocess for producing a mature spirit. In this embodiment, the processcomprises (a) contacting a first unmatured distilled spirit with wood ata temperature between about 140° F. and about 170° F. for a period oftime ranging from about 24 hours to about 336 to give a first distilledspirit mixture; (b) contacting a second unmatured distilled spirit withwood and actinic light at a wavelength spectrum ranging from 400 nm to1000 nm for at least 2 hours to give a second distilled spirit mixture;and (c) mixing the first and second distilled spirit mixtures to producethe mature spirit.

Step (a) of the process is conducted as described in Section (A)(i). Theresulting first distilled spirit mixture is not reacted with light.Separately, a second unmatured distilled spirit mixture is treated withactinic light as described in Section (A)(ii). The resulting seconddistilled spirit mixture is not treated by the thermal processing stepof Section (A)(i). Instead, the first distilled spirit mixture and thesecond distilled spirit mixture are mixed together.

The first distilled spirit mixture and the second distilled spiritmixture may be mixed in any ratio without limitation. In one embodiment,the ratio ranges between about 70:30 and about 30:70 of the firstdistilled spirit mixture to the second distilled spirit mixture. Inparticular embodiments, the ratio of the first distilled spirit mixtureand the second distilled spirit mixture is about 70:30, about 65:35,about 60:40, about 55:45, about 50:50, about 45:55, about 40:60, about35:65, or about 30:70. High concentration products may range from 99:1to 1:99, or, such as from a ratio of 95:5 to 5:95 of the first distilledspirit mixture to the second distilled spirit mixture.

The mixture of the first distilled spirit mixture and the seconddistilled spirit mixture is generally allowed to react for at least 1hour. Without being bound to any theory, it is believed that chemicalreactions occur during this time period that enhance the flavor profileover the flavor profile of the separately produced first distilledspirit mixture and the second distilled spirit mixture.

C. Simultaneous Heat and Light Processing

In still another embodiment, the present disclosure provides asimultaneous process for producing a mature spirit. In this embodiment,the process comprises contacting a unmatured distilled spirit with woodand maintaining the temperature between about 140° F. and about 170° F.for a period of time ranging from about 12 hours to about 336 hours, andat the same time, contacting the unmatured distilled spirit with actiniclight at a range of 400 nm to 1000 nm for at least 2 hours to give amature spirit. Thermal processing is conducted as described in Section(A)(i). Actinic light exposure is as described in Section (A)(ii).

D. Production of a Matured Spirit by Measuring Chemical Markers

In still another embodiment, the disclosure provides a process forproducing a spirit having characteristics of FIG. 5 or 6, as describedherein. The process comprises (a) obtaining a marker concentration of anester in a target matured distilled spirit thereby giving a targetmarker concentration, such as ethyl decanoate, as shown in FIG. 5 or 6,(b) contacting an unmatured distilled spirit with wood and processing asdescribed in Sections A-C to form a distilled spirit mixture, measuringthe marker concentration of the distilled spirit mixture, and (d)processing the distilled spirit mixture as described in Sections A-Cuntil the marker concentration of the distilled spirit mixture reachesthe target marker concentration.

Once the chemical marker concentration of the distilled sprit mixture isobtained it may be compared to the target marker concentration in orderto determine if heating and/or actinic light treating steps as describedin Sections A-C can be discontinued. When the target concentration isnot met, heating and/or light treatment steps are repeated. Thus, themethod provides a tunable process for producing a distilled spirithaving characteristics associated with, for example, FIG. 5 or 6. In oneembodiment, the chemical marker associated with a matured distilledspirit may be ethyl decanoate. The process disclosed above, however, isnot limited to ethyl decanoate, but can be any other ester that hashigher concentrations in a matured distilled spirit as compared to anunmatured distilled spirit. Esters are ideal markers for a heat processbecause the heat process excels at forming esters as opposed to othersemi-volatile compounds like sinapaldehyde.

Markers for the process include, but are not limited to ethyl decanoate,ethyl dodecanoate, ethyl octanoate, ethyl butyrate, and ethylhexadecanoate. In some embodiments, volatile esters can be used aschemical markers. But, semi-volatiles behave more predictably duringprocessing.

E. Wood Washing

In still another embodiment, the wood described in Sections A-D above iswashed prior to use in the method. Wood washing has the effect ofincreasing the concentrations of certain chemical markers that areimportant to the flavor of the matured spirit. In particular, woodwashing prior to conducting the method can lead to a higher ethylacetate concentration in the matured spirit.

Wood washing may be conducted by contacting the compound described belowwith wood. This contacting includes submerging the wood for a period oftime in a solution containing the compound or by pouring a solutioncontaining the compound over the wood.

In one embodiment, the wood is washed with a carboxylic acid containing1 to 10 carbon atoms. The carboxylic acid may be selected from, forexample, acetic acid, propionic acid, butanoic acid, pentanoic acid,hexanoic acid, heptanoic acid, octanoic acid, nonanoic acid, decanoicacid, branched carboxylic acids such as isobutyric acid, and aromaticacids such as benzoic acid and 2-phenylacetic acid.

The carboxylic acid may be diluted in water for the washing process. Forexample, the carboxylic acid can be a dilute solution having aconcentration from about 0.0001% and about 1% by volume, or about 1% toabout 10% by volume of the carboxylic acid, or the solution may beconcentrated to about 20% by volume, about 30% by volume, about 40% byvolume, about 50% by volume, about 60% by volume, about 70% by volume,about 80% by volume, about 90% by volume, or higher.

In one embodiment, the wood is washed with vinegar (i.e., a dilutesolution of acetic acid in water). When wood washing is conducted withany one of the processes described in Sections A-D, the final maturedspirit has higher ethyl acetate concentrations. For example, the ethylacetate concentration may be increased by 1.5× or more compared tospirit matured using this process without the vinegar washing. Thesehigher concentrations can give flavors characteristic to whiskeys suchas bourbon and rye whiskeys where higher ethyl acetate concentrationsare common.

F. Negative Pressure Processing

In combination with one or more processes disclosed in Section A-Eherein, air is percolated through a distilled spirit in a container witha headspace until the alcohol concentration of the distilled spirit isreduced. “Percolating” refers to gas aspirating or filtering graduallythrough a porous surface or substance. The air may be untreated air fromthe ambient atmosphere, or it may be filtered, dried, and ordeoxygenated air. Alternatively, the air may comprise one or more gasesselected from the group consisting of nitrogen, oxygen, argon, water,carbon dioxide, and helium, which are the principal gases of theterrestrial atmosphere.

In particular, the concentration of water in the air may be adjusted toattain a particular “relative humidity,” which is the ratio of theamount of water vapor actually present in the air to the greatest amountpossible at the same temperature. Without wishing to be bound by theory,a high relative humidity leads to a net loss of alcohol, whereas a lowrelatively humidity leads to a net loss of water. The relative humidity(RH) of the air may be selected from between about 0% and about 100%,such as between about 0% and about 10%, between about 10% and about 20%,between about 20% and about 30%, between about 30% and about 40%,between about 40% and about 50%, between about 50% and about 60%,between about 60% and about 70%, between about 70% and about 80%,between about 80% and about 90%, or between about 90% and about 100%.The relative humidity may be selected to mimic a geographical location,for example, Kentucky, Scotland, or Jamaica.

Generally, the air is introduced into to the container is at aboutatmospheric pressure. An air inlet at the bottom of the containerpermits the air to contact the distilled spirits. In large containers,the air inlet may be fluidly connected to a diffuser or perforated diskto distribute the air over a larger surface area, thus enhancing contactbetween the air and the distilled spirit.

During the process, the headspace of the container is under controllednegative gauge pressure. Although the container is open to theatmosphere or an air source, thereby allowing the air to percolatethrough, the headspace is enclosed by the top surface of the distilledspirit and the walls of the container, thereby allowing a negative gaugepressure to be exerted. Absolute pressure is zero-referenced against aperfect vacuum, so it is equal to gauge pressure plus atmosphericpressure. Gauge pressure is zero-referenced against ambient airpressure, so it is equal to absolute pressure minus atmosphericpressure, wherever the gauge is located. In stating the gauge pressure,negative signs may be omitted, but are used herein for clarity.

“Inch of mercury” (inches of Hg, inHg, or “Hg) is a unit of measurementfor pressure exerted by a column of mercury of 1 inch (25.4 mm) inheight at the standard acceleration of gravity. This simple gaugemeasures the difference in the levels of the mercury from 0 inches atatmospheric pressure up to 29.92 inches of Hg at the best vacuumattainable. Typically, this scale is shown as 0 to 30 inches of Hg ongauges, such a Bourdon dial gauges.

The range of gauge pressures used herein can and will vary. The gaugepressure of the headspace inside the container may be between about −25inHg and about −30 inHg, such as between about −25 inHg and about −25.5inHg, between about −25.5 inHg and about −26 inHg, between about −26inHg and about −26.5 inHg, between about −26.5 inHg and about −27 inHg,between about −27 inHg and about −27.5 inHg, between about −27.5 inHgand about −28 inHg, between about −28 inHg and about −28.5 inHg, betweenabout −28.5 inHg and about −29 inHg, between about −29 inHg and about−29.5 inHg, or between about −29.5 inHg and about −30 inHg. The gaugepressure may be between about −27 inHg and about −28 inHg. Inparticular, the gauge pressure may be about −27.75 inHg.

During the process, the distilled spirit may chill due to evaporativecooling, especially in large batches. As such, the temperature of thedistilled spirit may be heated during the process to hold thetemperature constant. Alternatively, the temperature may be lowered orraised relative to the ambient conditions. In these embodiments, thetemperature may range from between about 0° F. and about 140° F., suchas between about 0° F. and about 10° F., between about 10° F. and about20° F., between about 20° F. and about 30° F., between about 30° F. andabout 40° F., between about 40° F. and about 50° F., between about 50°F. and about 60° F., between about 60° F. and about 70° F., betweenabout 70° F. and about 80° F., between about 80° F. and about 90° F.,between about 90° F. and about 100° F., between about 100° F. and about110° F., between about 110° F. and about 120° F., between about 120° F.and about 130° F., or between about 130° F. and about 140° F. Thetemperature may be greater than 0° F. The temperature may be less than140° F.

The volume of distilled spirits used in the process can and will vary.For example, the volume may range from about 100 mL to about 10,000 L,such as between about 100 mL and about 500 mL, between about 500 mL andabout 1 L, between about 1 L and about 1.5 L, between about 1.5 L andabout 2 L, between about 2 L and about 5 L, between about 5 L and about10 L, between about 10 L and about 50 L, between about 50 L and about100 L, between about 100 L and about 500 L, between about 500 L andabout 1,000 L, between about 1,000 L and about 2,000 L, between about2,000 L and about 5,000 L, or between about 5,000 L and about 10,000 L.The volume may be greater than about 100 mL. The volume may be less thanabout 10,000 L. The volume may be about 325 mL. The volume may be about750 mL. The volume may be about 1.5 L.

The process disclosed herein decreases the concentration of alcoholwithin the distilled spirit, and thereby selectively removes the mostvolatile organic compounds and azeotropes and/or increases theconcentration of desirable chemical markers. The disclosed process isvery sensitive and is preferably monitored carefully to the targetalcohol concentration. (As used throughout this disclosure, “alcohol”without further qualification takes its common meaning of “ethanol.”)The alcohol concentration of the distilled spirit may be determinedduring the process using an in-line density meter connected to thecontainer. In these embodiments, the vacuum chamber should be fittedwith an in-line density meter to carefully monitor the changes inalcohol percentage in the spirit, allowing for very precise processing.An in-line density meter is critical to scaling the system to largervolumes. If the disclosed process is run too long, the distilled spiritsbecomes very bitter. If the disclosed process is run for too short of atime, the distilled spirit retains chemical markers which gives theperception of heat to a consumer.

The disclosed process can be used on either full strength spirits orbottling strength spirits with the adjustments to the target alcoholconcentration, as described herein. The unmatured distilled spirit, asdescribed herein, has an alcohol content of at least 50% by volume. Insome embodiments, the alcohol content of the unmature distilled spiritis between 40% and 95.5% by volume. “Full strength” is the strength ofdistilled spirit straight from the cask (barrel) with no water added.Full strength spirits typically have an alcohol concentration of greaterthan 60% by volume, such as greater than 65%, as greater than 70%, asgreater than 75%, as greater than 80%, as greater than 85%, or asgreater than 90% by volume. The initial concentration of alcohol may bebetween about 40% and about 95.5% by volume. “Bottling strength” refersto the concentration to which distilled spirits are diluted to whentransferring from the cask (barrel) to a bottle, which is between about40% and about 57% by volume for most bottled spirits, such as betweenabout between about 40% and about 45% by volume, between about 45% andabout 50% by volume 50% and about 55% by volume, or between about 52%and about 57% by volume.

As such, the alcohol concentration of full strength distilled spirit maybe reduced by between about 1% and about 2% by volume, such as betweenabout 1.1% and about 1.2% by volume, between about 1.2% and about 1.3%by volume, between about 1.3% and about 1.4% by volume, between about1.4% and about 1.5% by volume, between about 1.5% and about 1.6% byvolume, between about 1.6% and about 1.7% by volume, between about 1.7%and about 1.8% by volume, between about 1.8% and about 1.9% by volume,or between about 1.9% and about 2.0% by volume. As such, the alcoholconcentration of bottle strength distilled spirit may be reduced bybetween about 0.3% and about 1% by volume, such as between about 0.3%and about 0.4% by volume, between about 0.4% and about 0.5% by volume,between about 0.5% and about 0.6% by volume, between about 0.6% andabout 0.7% by volume, between about 0.7% and about 0.8% by volume,between about 0.8% and about 0.9% by volume, or between about 0.9% andabout 1.0% by volume.

Unlike traditional methods, which lose between about 30% and about 50%of the volume to evaporation in the barrelhouse, the disclosed processremoves less than about 20% of the total volume of the spirit, whilecreating substantially the same flavor characteristics as associatedwith very old spirits. For example, the disclosed process may removeless than about 20% of the total volume of the spirit, such as less thanabout 19%, less than about 18%, less than about 17%, less than about16%, less than about 15%, less than about 14%, less than about 13%, lessthan about 12%, less than about 11%, less than about 10%, less thanabout 9%, less than about 8%, less than about 7%, less than about 6%,less than about 5%, less than about 4%, less than about 3%, less thanabout 2%, or less than about 1% of the total volume of the spirit. Asdescribed above, the parameters selected for the process determinewhether the net loss from the lost volume is net water or net alcohol.

One aspect of the present disclosure provides a process for maturing adistilled spirit using sequential pressure processing. In this regard,the process comprises the steps describe above, wherein the distilledspirit in step (a) begins with an alcohol concentration greater than 60%by volume. The process then further comprises (b) diluting the distilledspirit of step (a) with water to an alcohol concentration between about50% and about 55% by volume, and then (c) percolating air through thediluted distilled spirit in the container with the headspace at a gaugepressure between about −25 inHg and about −30 inHg until the alcoholconcentration of the diluted distilled spirit is reduced an additionalamount of between about 0.3% and about 1% by volume. The alcoholconcentration of the distilled spirit may be determined during theprocess using an in-line density meter connected to the container.

As in the first sequence of pressure treatment, the gauge pressure maybe between about −27 inHg and about −28 inHg, such as at about −27.75inHg. Any pressure described herein is sufficient. The temperature ofthe distilled spirit may be held constant during the step (c) above.

In particular, the present disclosure provides a process for maturing adistilled spirit. (a) Air percolated through a distilled spirit in acontainer with a headspace at a gauge pressure between about −27 inHgand about −28 inHg until alcohol concentration of the distilled spiritis reduced by between about 1% and about 2% by volume, as determined byan in-line density meter connected to the container. In this process,the total volume of the spirit is reduced by about 10% or less. Thedistilled spirit begins step (a) with an alcohol concentration greaterthan 60% by volume. And then optionally, (b) air is percolated throughthe distilled spirit of step (a) in the container with the headspace ata gauge pressure between about −27 inHg and about −28 inHg until thealcohol concentration of the distilled spirit is reduced by anadditional amount of between about 0.3% and about 1% by volume, asdetermined by the in-line density meter. And then (c) the distilledspirit of step (b) is diluted with water to an alcohol concentrationbetween about 50% and about 55% by volume. And then (d) air ispercolated air through the diluted distilled spirit in the containerwith the headspace at a gauge pressure between about −27 inHg and about−28 inHg until the alcohol concentration of the diluted distilled spiritis reduced by an additional amount of between about 0.3% and about 1% byvolume, as determined by the in-line density meter.

As described elsewhere in this disclosure, the distilled spirit may beselected from the group consisting of sugar cane spirits, grain spirits,fruit spirits, or agave spirits. Alternatively, the distilled spirit maybe selected from the group consisting of rum, tequila, mescal, whiskey,brandy, gin, and vodka.

The gauge pressure in each of steps (a) and (c) may be about −27.75inHg. The temperature of the distilled spirit may be held constantduring each of steps (a), (b), and (c).

The concentration in the distilled spirit may be decreased for one ormore chemical markers selected from the group consisting of methanol,C₂-C₆ fatty acids, and C₂-C₆ fatty acid esters. Alternatively or inaddition, the concentration in the distilled spirit may be increased forone or more chemical markers selected from the group consisting ofvanillin, phenylated esters, C₇-C₂₄ fatty acid esters, and phenolicaldehydes. In particular, the distilled spirit may be characterized byan increase in concentration of sinapaldehyde, ethyl dodecanoate, andethyl decanoate. The distilled spirit may characterized by an increasein concentration of sinapaldehyde. The total loss of volume of distilledspirits during the process may be less than about 20%.

Optionally, the spirit produced by the process described herein may befollowed by one or more additional pressure processing steps. In oneembodiment, the sequential process may be repeated until a desiredchemical marker profile is obtained.

The present disclosure also provides a distilled spirit producedaccording to a process described herein.

The compounds described herein have asymmetric centers. Compounds of thepresent disclosure containing an asymmetrically substituted atom may beisolated in optically active or racemic form. All chiral,diastereomeric, racemic forms and all geometric isomeric forms of astructure are intended, unless the specific stereochemistry or isomericform is specifically indicated.

When introducing elements of the present disclosure or theembodiments(s) thereof, the articles “a,” “an,” “the,” and “said” areintended to mean that there are one or more of the elements. The terms“comprising,” “including,” and “having” are intended to be inclusive andmean that there may be additional elements other than the listedelements.

Having described the disclosure in detail, it will be apparent thatmodifications and variations are possible without departing from thescope of the disclosure defined in the appended claims.

Examples

The following examples are included to demonstrate certain embodimentsof the disclosure. It should be appreciated by those of skill in the artthat the techniques disclosed in the examples represent techniquesdiscovered by the inventors to function well in the practice of thedisclosure. Those of skill in the art should, however, in light of thepresent disclosure, appreciate that many changes can be made in thespecific embodiments that are disclosed and still obtain a like orsimilar result without departing from the spirit and scope of thedisclosure, therefore all matter set forth is to be interpreted asillustrative and not in a limiting sense.

Instrumentation

Gas Chromatography Mass Spectrometry (GCMS) Data was obtained using aShimadazu GCMS Model QP2010 with a Restek Column—Rxi-5Sil MS, 30 meter,0.24 mmID, 0.24 umdf. Program conditions were as follows:

TABLE 1 Analytical Line 1 # of Rinses with Presolvent :1 # of Rinseswith Solvent(post) :5 # of Rinses with Sample :1 Plunger Speed(Suction):Middle Viscosity Comp. Time :5.0 sec Plunger Speed(Injection) :HighSyringe Insertion Speed :High Injection Mode Normal Pumping Times :3Inj. Port Dwell Time :10.0 sec Terminal Air Gap :No Plunger WashingSpeed :High Washing Volume :6 uL Syringe Suction Position −2.0 mmSyringe Injection Position :0.0 mm Solvent Selection :All A, B, C

TABLE 2 GC PARAMETERS Column Oven Temp. :35.0° C. Injection Temp.:265.0° C. Injection Mode :Split Flow Control Mode :Linear VelocityPressure :56.0 kPa Total Flow :23.9 mL/min Column Flow :1.12 mL/minLinear Velocity :38.0 cm/sec Purge Flow :0.5 mL/min Split Ratio :20.0High Pressure Injection :OFF Carrier Gas Saver :ON Carrier Gas SaverSplit Ratio  :5.0 Carrier Gas Saver Time :10.00 min

TABLE 3 OVEN TEMP. PROGRAM Rate Temperature (° C.) Hold Tim (min) 35.05.00 16.00 300.0 1.44

TABLE 4 MS PARAMETERS IonSourceTemp :220.00° C. Interface Temp. :280.00°C. Solvent Cut Time :1.80 min Detector Gain Mode :Relative Detector Gain:0.20 kV Threshold  :500 Start Time :1.80 min End Time :23.00 min ACQMode :Scan Event Time :0.50 sec Scan Speed :1000 Start m/z  :35.00 Endm/z  :500.00

Comparative Example 1: Fresh Rum

A sample of fresh, unmature pot distilled rum was analyzed by GCMS. FIG.1 shows the semi-volatile fingerprint of an un-aged pot distilled rum.This is largely defined by a lack of activity for compounds having aretention time ranging from 5 to 30 minutes. Noteworthy characteristicsinclude, but are not limited to, the starting height of peak 1corresponding to acetyl, peak 2 corresponding to ethyl decanoate, andpeak 3 corresponding to ethyl dodecanoate. The absence of a peak forsinapaldehyde, which is described further in later examples, isnoteworthy. FIG. 1 also shows an absence of white noise in thechromatogram starting at the 6 minute retention time point.

Concentration of ethyl acetate was measured by direct injection massspectrometry. The concentration of ethyl acetate was shown to be about110,000 μg/L.

Comparative Example 2: Rum Aged for 33 Years by Conventional AgingProcess

A sample of a commercially-available rum which has been aged for 33years by conventional aging processes was also analyzed by GCMS. FIG. 2illustrates a semivolatiles profile characteristic of 33 year aged potdistilled rums. Key characteristics include the high acetal spike(peak 1) the high ethyl decanoate spike (peak 2) the high ethyldodecanoate spike (peak 3) and the high sinapaldehyde spike (peak #4).The relative heights of peaks 2, 3, and 4 in relation to each other isalso important. Organoleptically maintaining this approximate ratio ofpeak heights to each other proved significant for creating the flavorcharacteristics associated with aged rum. Further noteworthy is thecluster of medium level peaks centered on the 15-minute mark (thought tobe caramel additives and found to include significant amounts ofglucose—this phenomena was also observed in known adulterated rum).

The critical differences between the un-aged rum and the 33-year-oldrum, that were ascertainable in the semi-volatile chromatograms includedthe presence of sinapaldehyde (not found in the white rum) alongsidepeaks showing significantly elevated ethyl decanoate and ethyldodecanoate levels (both of which are found in the white rumcharacterized by relatively low peak values). Finally a significantlayer of “white noise” (representing a complex mixture of manysemi-volatile compounds) lined the bottom of the chromatogram in the33-year-old rum and was absent in the un-aged rum.

Concentration of ethyl acetate was measured by direct injection massspectrometry. The concentration of ethyl acetate was shown to be about770,000 μg/L. A more typical reading for ethyl acetate in a 33 year-oldsample is 200,000 μg/L.

Comparative Example 3: Heat Only Process

Otherwise unprocessed heavy pot distilled rum was added to a stainlesssteel tank and mixed with charred oak slabs and heated to between 150°F. and 170° F. Temperature was held in that range for 48 hours. FIG. 3shows the GCMS chromatogram of the resulting product. The GCMS showspromising (but inadequate) developments of acetyl (peak 1) ethyldecanoate (peak 2), ethyl dodecanoate (peak 3) and sinapaldehyde (peak4). It also shows the development of some white noise. Overall thissample did not produce all of the organoleptic properties displayed inaged rum. The flavor and aroma of the sample was abnormally thin andlacked the smoky/woody flavors found in the 33 year-old sample.Qualitatively it was unable to meet two of the key chemical markercriteria for the production of aged rum. As can be seen, the white noiselevel was low. The ethyl dodecanoate (peak 3) and sinapaldehyde (peak 4)failed reach peak heights similar to the ethyl decanoate (peak 2).

Concentration of ethyl acetate was measured by direct injection massspectrometry. The concentration of ethyl acetate was shown to be about38,000 μg/L.

Comparative Example 4: Actinic Light Only Process

Otherwise unprocessed heavy pot distilled rum was placed in a sealedflint glass jar along with charred oak slabs and placed in a greenhousefor 30 days. The sample was not subjected to any heat treatment. Thesample was analyzed by GCMS. The GCMS shows significant development ofacetyl (peak 1) ethyl decanoate (peak 2), ethyl dodecanoate (peak 3) andsinapaldehyde (peak 4). It also shows the development of the level ofwhite noise expected in a mature spirit. But, this sample did notproduce the organoleptic properties displayed in aged rum. It wasextremely bitter. Qualitatively it was unable to meet one key chemicalmarker criteria for the production of an aged spirit. The sinapaldehyde(peak 4) was extremely high. It was hypothesized that the extreme levelof sinapaldehyde was partially causing the bitterness along with someother observed and abnormally high peaks including furfural (peak 5) andsyringaldehyde (peak 6).

Concentration of ethyl acetate was measured by direct injection massspectrometry. The concentration of ethyl acetate was shown to be about62,000 μg/L.

Example 5: Mixed Batch Heat and Actinic Light Process

Otherwise unprocessed heavy pot distilled rum was added to a stainlesssteel tank and mixed with charred oak slabs and heated to between 150°F. and 170° F. Temperature was held in that range for 48 hours.Separately, an otherwise unprocessed heavy pot still rum was placed in asealed flint glass jar along with charred oak slabs and placed in agreenhouse for 30 days. The product of the heat treatment and theproduct of the light treatment were then mixed together with a ratio of60% of the heat process product and 40% of the actinic light processedrum. This mixture was allowed to react for 24-48 hours. After this timeperiod, the resulting product was analyzed by GCMS. The GCMSchromatogram is shown in FIG. 5. The chromatogram shows some unexpectedresults along with major developments. The acetyl concentration (peak 1)unexpectedly fell to a concentration lower than that of either of itsconstituent parts (FIGS. 3 and 4). But, the acetal level was stillelevated in comparison to the unprocessed rum (FIG. 1) by a factor of1.75×. The furfural concentration (peak 5) and syringaldehydeconcentration (peak 6) unexpectedly fell sharply correcting theoverabundance of these compounds displayed in the actinic light-treatedrum (FIG. 4). The ethyl decanoate concentration (peak 2) unexpectedly(and counterproductively) fell to levels lower than those observed ineither of the constituent components—yet the peak still remained morethan 3× higher than the starting concentration in the unprocessed rumsatisfying our minimum criteria for an aged spirit. Ethyl dodecanoate(peak 3) was unaffected by combining the products. Critically, thesinapaldehyde (peak 4) fell to a concentration lower than expected giventhe extremely high peak found in the actinic light reacted product (FIG.4). The “white noise” fell significantly and unexpectedly, failing tofully satisfy criteria for an aged spirit. Despite the failure of thisproduct to fully meet some markers of the 33-year-old spirit, thisproduct did produce the organoleptic properties displayed in aged rum,albeit a highly idiosyncratic aged rum. It did not display any of theextreme bitterness found in the actinic light reacted rum (FIG. 4), orthe thinness of flavor displayed in the temperature treated rum (FIG.3). It was observed that the peak heights of ethyl decanoate, ethyldodecanoate, and sinapaldehyde were all elevated and had come closer toaligning than had been possible in either the heat-treated product orthe actinic light-treated product alone. Therefore the mixture of thetwo products had produced a final product that approached meeting all ofthe key chemical markers outlined in our definition of a mature spirit.

Concentration of ethyl acetate was measured by direct injection massspectrometry. The concentration of ethyl acetate was shown to be about170,000 μg/L.

Example 6: Sequential Temperature and Light Processing

An otherwise unprocessed heavy pot distilled rum was added to astainless steel tank and mixed with charred oak slabs and heated tobetween 150° F. and 170° F. Temperature was held in that range for 48hours. The resulting product was then placed in a sealed flint glass jaralong with charred oak slabs and placed in front of a 500-W halogen bulbfor 3 days. Seventy glass jars are placed on a shelf surrounded by atotal of 20 lights. The lights were toggled on and off in 2-4 hourcycles to prevent boiling. The resulting product was then placed in astainless steel tank and mixed with charred oak slabs and heated tobetween 150° F. and 170° F. Temperature was held in that range for 48hours. The resulting product was analyzed with GCMS.

FIG. 6 shows the GCMS chromatogram from a rum sample that has beenprocessed with both heat and light in accordance with Example 6. Itshows some unexpected results along with major developments. Unlike themixture of the heat and actinic light-treated rum described in FIG. 5,the acetyl concentration (peak 1) is as high as it is in the actiniclight reacted rum (FIG. 4) more than 3× the starting concentration foundin the unprocessed rum (FIG. 1) satisfying the acetyl chemical markercriteria for an aged spirit. The furfural concentration (peak 5) doesnot exhibit the overabundance displayed in the actinic light-treated rum(FIG. 4). The ethyl decanoate concentration (peak 2) shows a peak height25%+/−higher than that found in the mixture of heat treated rum andactinic light reacted rum described in FIG. 5. The peak shows a relativeconcentration roughly 5× higher than the starting concentration in theunprocessed rum satisfying our minimum ethyl decanoate marker criteriafor an aged spirit. The ethyl dodecanoate (peak 3) peak height wasidentical to that found in the mixture described in FIG. 5 and lines upalmost identically with the ethyl decanoate concentration. Thesinapaldehyde (peak 4) fell slightly from the light/heat mixture rumdescribed in FIG. 5 critically aligning with the ethyl decanoate (peak2), and the ethyl dodecanoate (peak 3) satisfying the elusive chemicalmarker criteria of having peaks 2, 3, and 4 roughly aligned. The “whitenoise” peaks also rose (as compared to the mixture product displayed inFIG. 5) as a consequence of this modified process satisfying thatchemical marker criteria for the production of an aged spirit. As isexpected from reading the chromatogram, this product did produce theorganoleptic properties displayed in aged rum. It did not display any ofthe extreme bitterness found in the actinic light reacted rum (FIG. 4),or the thinness of flavor displayed in the temperature treated rum (FIG.3). It was observed that the peak heights of ethyl decanoate, ethyldodecanoate, and sinapaldehyde were all elevated and roughly aligned ina way that had not been possible in either the heat-treated product orthe actinic light-treated product, or even the mixture of the two (shownin FIG. 5). This process had successfully satisfied all of the keychemical markers outlined in our definition of a mature spirit,elegantly solving the industries “30 years in a barrel” problem. Itincidentally and beneficially triggered a marked reduction in ethylacetate concentrations, shown experimentally to be greater than 60% overthe batch process (FIG. 5). The process also produced no evaporation ofthe finished product as would be expected in conventional barrel aging.The finished product not only mimicked the key marker ratios atraditionally aged product, but ultimately improved the process byshortening the time to maturity, eliminating the evaporation, andreducing the ethyl acetate.

Concentration of ethyl acetate was measured by direct injection massspectrometry. The concentration of ethyl acetate was shown to be about59,000 μg/L.

While specific embodiments have been described above with reference tothe disclosed embodiments and examples, such embodiments are onlyillustrative and do not limit the scope of the disclosure. Changes andmodifications can be made in accordance with ordinary skill in the artwithout departing from the disclosure in its broader aspects as definedin the following claims.

What is claimed is:
 1. A process for producing a mature spiritcomprising: (a) providing heat to a mixture consisting essentially of anunmatured distilled spirit and wood, to maintain a temperature betweenabout 140° F. and about 170° F. for a period of time ranging from about24 hours to about 336 hours to give a distilled spirit mixture; then (b)contacting the distilled spirit mixture with wood and actinic light at awavelength spectrum ranging from 400 nm to 1000 nm for at least twohours to give an actinic light-treated distilled spirit mixture; andthen (c) providing heat to the actinic light-treated distilled spiritmixture produced in step (b) to maintain a temperature between about140° F. and about 170° F. for a period of time ranging from about 12hours to about 336 hours to produce the mature spirit; and then whereinsteps (a), (b), and (c) are performed sequentially.
 2. The process ofclaim 1, wherein the unmatured distilled spirit is selected from thegroup consisting of sugar can spirits, grain spirits, fruit spirits, oragave spirits.
 3. The process of claim 1, wherein the unmatureddistilled spirit is selected from the group consisting of rum, tequila,mescal, whiskey, brandy, gin, and vodka.
 4. The process of claim 1,wherein the mature spirit is characterized by amounts of sinapaldehyde,ethyl dodecanoate, and ethyl decanoate that are substantially similar tothe relative proportions shown in FIG. 6, as measured by GCMS.
 5. Theprocess of claim 1, wherein the mature spirit has an ethyl acetateconcentration of about 59,000 μg/L.
 6. The process of claim 1, whereinsteps (a) and (c) are maintained at a temperature between about 140° F.and about 150° F. for a period of time ranging from about 168 hours toabout 226 hours.
 7. The process of claim 1, wherein steps (a) and (c)are maintained at a temperature between about 150° F. and about 160° F.for a period of time ranging from about 24 hours to about 72 hours. 8.The process of claim 1, wherein the process further comprises: (e)contacting the mature spirit of step (c) with wood and actinic light ata wavelength spectrum ranging from 400 nm to 1000 nm for at least twohours.
 9. The process of claim 8, where the process further comprises:(f) heating with wood at a temperature between about 140° F. and about170° F. for a period of time ranging from about 24 hours to about 336hours after step (e).